Catalytic or photocatalytic preparation method of parylene af4
a technology of parylene af4 and photocatalysis, which is applied in the preparation of halogenated hydrocarbons, group 5/15 element organic compounds, organic chemistry, etc., can solve the problems of increasing the preparation cost and not being suitable for mass production, and achieve the effect of significantly increasing the production capacity of parylene af4
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Benefits of technology
Problems solved by technology
Method used
Image
Examples
embodiment 1
[0021]This embodiment involves providing a 250 ml three-necked bottle and purging with nitrogen, then adding 75 ml of DMAC solvent, 15.68 g (0.24 mol) of reducing agent zinc powder, and 0.21 g (3.5 mmol) of catalyst KF, stirred and preheated to 120° C. Then 29.64 g (0.12 mol) of reactant CH3 is added dropwise to the reaction bottle, and the reaction temperature is gradually increased to 135° C., the feeding time is about 2 hours and the reaction is continued for 3 hours. The crude product is filtered and washed by DMAC. The double bond-containing byproduct in filtrate is oxidized by potassium permanganate, and the filtrate is concentrated and water is added to the resulting crude solid in order to remove the inorganic substances. The crude solid obtained from filtration and recrystallized in chloroform (CHCl3) to obtain 8.43 g of pure parylene AF4 (purity 99.5%, yield 40.28%). The parylene AF4 product is confirmed by analysis: the molecular weight of 352.0 g / mol is confirmed by GC / M...
embodiment 2
[0022]In this embodiment of the present invention, a 250 ml three-necked bottle is provided and purged with nitrogen, then 50 ml of DMAC solvent is added, 7.84 g (0.12 mol) of reducing agent zinc powder, and 0.10 g (0.6 mmol) of catalyst stirred and preheated to 120° C. Then the mixture of 14.82 g (0.06 mol) of reactant CFB and 1.95 g (0.006 mol) of reactant BFB is added dropwise to the reaction bottle, and the reaction temperature is gradually increased to 140° C., the feeding time is about 1 hour and the reaction is continued for 3 hours. The crude product is purified and analyzed by the same methods of embodiment 1 and 3.58 g of parylene AF4 is obtained (purity 99.63%, yield 31.0%).
embodiment 3
[0023]Provide a 250 ml three-necked bottle and purge with nitrogen, then add 150 ml of DMSO solvent, 7.84 g (0.12 mol) of reducing agent zinc powder, and 0.10 g (0.6 mmol) of catalyst KI, stirred and preheated to 120° C. Then 14.82 g (0.06 mot) of reactant CFB is added dropwise to the reaction bottle, and the reaction temperature is gradually increased to 131° C., the feeding time is about 1 hour and the reaction is continued for 3 hours. The crude product is purified and analyzed by the same methods of embodiment 1 and parylene AF4 is obtained with 99.34% of purity and 26.7% of yield.
PUM
| Property | Measurement | Unit |
|---|---|---|
| Temperature | aaaaa | aaaaa |
| Polarity | aaaaa | aaaaa |
| Weight ratio | aaaaa | aaaaa |
Abstract
Description
Claims
Application Information
Login to View More 


